反応 #339043

反応方程式

compound

7-[(3RS,5SR)-4-(Azidoacetyl)-3,5-dimethylpiperazin-1-yl]-1-cyclopropyl-N-(2,4-dichlorobenzyl)-6-fluoro-8-methoxy-4-oxo-1,4-dihydroquinoline-3-carboxamide hydrochloride

triphenylphosphine

→

1-Cyclopropyl-N-(2,4-dichlorobenzyl)-6-fluoro-7-[(3RS,5SR)-4-glycyl-3,5-dimethylpiperazin-1-yl]-8-methoxy-4-oxo-1,4-dihydroquinoline-3-carboxamide hydrochloride

溶媒

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   workup.ADDITIONare added dropwise
2. 2
   温度the reaction mixture is warmed to room temperature
3. 3
   その他For the work-up the solvent is removed completely on a rotary evaporator
4. 4
   その他after fine purification by column chromatography on silica gel 60 (eluent: dichloromethane:ethanol 90:10)
5. 5
   濃縮concentrating the fractions
6. 6
   workup.ADDITIONwith the addition of hydrochloric acid 24 mg of the target compound
7. 7
   その他are obtained

実験手順

46.0 mg (0.07 mmol) of the compound of Example 82A are provided in 2 ml of tetrahydrofuran, the solution is cooled to 0° C., 21.1 mg (0.08 mmol) of triphenylphosphine, dissolved in 1 ml of tetrahydrofuran are added dropwise, the reaction mixture is warmed to room temperature and stirred over night at this temperature. For the work-up the solvent is removed completely on a rotary evaporator, the residue is prepurified by preparative RP-HPLC (Method 6) and after fine purification by column chromatography on silica gel 60 (eluent: dichloromethane:ethanol 90:10) and concentrating the fractions with the addition of hydrochloric acid 24 mg of the target compound are obtained.

出典